CN1185036C - Method for preparing concentrated solution - Google Patents
Method for preparing concentrated solution Download PDFInfo
- Publication number
- CN1185036C CN1185036C CNB001333569A CN00133356A CN1185036C CN 1185036 C CN1185036 C CN 1185036C CN B001333569 A CNB001333569 A CN B001333569A CN 00133356 A CN00133356 A CN 00133356A CN 1185036 C CN1185036 C CN 1185036C
- Authority
- CN
- China
- Prior art keywords
- distillation column
- falling film
- solution
- film evaporator
- boiling point
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Process for the manufacture of a concentrated solution, like a concentrated aqueous hydrogen peroxide solution, by distillation and evaporation of a dilute solution, in which the distillation and the evaporation are carried out in two distinct pieces of equipment which are easy to dismantle and to transport. Aqueous hydrogen peroxide solutions having a concentration of at least 90% are obtainable.
Description
Technical field
The present invention relates to a kind of method for preparing concentrated solution under the condition of safety economy, it is to adopt a kind of device that is easy to remove and transport to carry out.The invention still further relates to the inventive method and produce the purposes that concentrates superoxol, and relate to these spissated superoxols.
Background technology
Knew already that some concentrated solution can be used for explosion caused decomposition as concentrating superoxol.The method of this class concentrated solution of known preparation mostly is to be begun by dilute solution, and adopts evaporation and/or distillation technique.In concentration process, because when temperature and/or concentration increase, the blast energy needed reduces, so along with the increase of temperature and/or concentration, the possibility of explosive decomposition also increases, therefore, it is very crucial.And the degree that this class may be exploded depends on the accumulation of concentrated solution, and therefore, it is the key that is used for the concentration process device.
Adopt the resulting ultimate density of these class methods, normally limited, this is not only owing to the safety factor of having mentioned, and is because the suffered thermodynamical restriction of these class methods, its pressure and temperature condition depends on Design of device, particularly depends on the design of distillation tower.
In addition, this class currently known methods also is very high at the cost aspect investment and/or the energy consumption.
At last, be used for the known devices of these class methods, normally under vacuum condition, operate.Consequently, if should need to remove and/or transportation, their assembling and compactness are very important, and may become a problem.For example, for spissated hydrogen peroxide, for fear of this spissated solution of transportation, concentrating unit being positioned near the place to use of hydrogen peroxide, is very easily.
Some known method has solved above-mentioned one or more in the problem of mentioning, but they all can not address all of these issues.
GB668874 relates to a kind of method for preparing highly enriched superoxol, prepares by the distillation dilute solution, wherein, evaporates in two overlapping dishes from the distillatory high boiling fraction.The shortcoming of this method is that it adopts at least two horizontal liquid layers to operate.The pressure drop meeting that these liquid layers cause improves the boiling temperature of this liquid, thereby can increase the possibility of explosive decomposition.And this horizontal liquid layer can cause accumulation of fluid in the high zone of strength of solution.Another shortcoming of GB668874 method is the high calorie consumption of vaporizer.
EP835680 relates to a kind of by at least one fill area and the distillation column that vaporizer is formed of being positioned on the same longitudinal axis, and it comprises at least two vaporizers and/or two condensers.Adopt two vaporizers and/or condenser in this class device, comparatively complexity and cost are more expensive.And it can not provide and be used for preventing concentrated solution accumulative element.Therefore, it preferably is used for preparing concentration and is lower than 70% solution.Also have, it is difficult to remove and/or transport very much.
Summary of the invention
The objective of the invention is provides a kind of method for preparing concentrated solution under the condition of safety economy in order to overcome the deficiency in the currently known methods, adopts a kind ofly to be easy to remove and be transported near the device the employed place of concentrated solution and to realize.
For this purpose, the present invention relates to a kind ofly prepare the method for concentrated solution from dilute solution, wherein, distillation and evaporation are carried out in a distillation column and a vaporizer, and they form two distinct device features, can easily remove and transport.
These two device features are distinct facts, mean that they all contain a bottom and top layer, and fluid can therefrom flow through, and they can work alone.
Adopt two distinct device feature distillation columns and vaporizer, its major advantage is that the more used single post of whole device is easy to remove and transportation more.Use the device of two completely different parts,, astoundingly, with the problem that can not cause being caused by the liquid gathering, and their expectations in the associating parts are to take place, particularly when they contain the area of reduction.
In a preferred embodiment of the invention, being connected between described distillation column and vaporizer, realize by a divider, its cross-sectional area at narrow place less than the cross-sectional area of described distillation column.
The cross section of described distillation column is according to long-pending calculating of average cross-section of the horizontal zone of effective fill area of this post, does not comprise above-mentioned bottom and top.
Divider of the present invention can be the liquid dispenser of any known kind, and it can form thin film along the wall of falling film evaporator, and condition is the geometrical shape that it has above-mentioned needs.Adopt an end to have big cross section and the other end has the divider of smaller cross-sectional area, can obtain good result.In this case, maximum cross section is to be connected with described distillation column, and minimum cross section is connected with described falling film evaporator.
Preferably, this distillation column and vaporizer are to adopt such mode to assemble, and it can allow liquid, only under action of gravity, just can flow to the described vaporizer from this distillation column.
More preferably, described distillation column is mounted on the top layer of this vaporizer, and the axle of two device features in line.
Method of the present invention preferably adopts a kind of feeding unit, and it is positioned at a certain position or a plurality of position of distillation column.This feeding unit for example is the 2/3 top place that is positioned at this post.
This distillation column can be filled with the fractionation plant or the filler of suitable number.These transposition can be selected from the known multiple fractionation plant of distillation column technician, for example porous plate, valve tray, bubble cap plate and multiple filler for example, Raschig ring, Pall ring and wrought mat.Structured packing such as structured packing-SULZER BX type is preferred.
Vertical surface preferably within the distillation column is to prevent accumulation of fluid.The bottom of distillation column preferably also is to be designed to prevent any accumulation of fluid.
In another advantageous embodiments of the present invention, described vaporizer is a kind of falling film evaporator.The falling film evaporator of this embodiment is generally a kind of long tube formula vertical evaporator, wherein, flow into the top layer of this pipe continuously from the effusive concentrated solution of distillation column bottom, and flows down along its wall with the form of film.The number of described pipe and size can make the delay of hydrogen peroxide in vaporizer minimize.
Preferably, method of the present invention adopts a kind of heating unit, is used for described falling film evaporator, and hot water circulates therein.
Method of the present invention also can adopt a water cooler and a divider that is used to be connected described falling film evaporator and this water cooler.This water cooler is preferably the falling film type water cooler.It can adopt heat-transfer medium commonly used arbitrarily to cool off.Preferably, this heat-eliminating medium is water and/or ethylene glycol.
This installs the building material of all parts, and with regard to the corrosion and stability of product, they must can coexist fully with solution.Aluminium, glass and fluoropolymer are preferable material.
Method of the present invention can be used to prepare any spissated solution.It is particularly suitable for being used for preparing spissated aqueous hydrogen peroxide solution, especially concentration and is at least 80% weight, particularly concentration and is at least 90% superoxol.Normally, concentration is at most 98% weight.
According to a preferred embodiment of the present invention, described method comprises the steps:
(a) a certain position on distillation column or a plurality of position input dilute solution;
(b) in this distillation column, distill described dilute solution, obtain the lower boiling gaseous fraction of solution at the top of described distillation column, obtain the high boiling point liquid fraction of solution in the bottom of described distillation column;
(c) through divider, the high boiling point liquid fraction of described solution to be transferred to the described vaporizer from described distillation column bottom, it is a kind of falling film evaporator;
(d) the high boiling point liquid fraction of concentrated described solution in described falling film evaporator; With
(e) collect spissated solution in the bottom of described falling film evaporator.
Filling extract rectification or enrichment region that described dilute solution feed entrance point will be lower than the filler stripping or the washing section of feed points usually and be higher than feed points are separated.
In the method for the invention, preferably there is not the recirculation of liquid.
Distillation is mainly carried out under reduced pressure, to limit the boiling temperature of the described high boiling point liquid fraction that must evaporate.Usually, described pressure is lower than 40 torrs.The peak pressure that often adopts in the still-process is 10 torrs.Pressure in the still-process is usually above about 5 torrs.The minimum pressure of 3 torrs is also usually observed in still-process.Normally, the distillation column bottom temp is lower than 50 ℃.The bottom temp that is lower than 40 ℃ is more suitable.Usually, described bottom temp should be higher than 0 ℃.
Illustrated as mentioned, in falling film evaporator of the present invention, the number of described pipe and size should make the accumulation of fluid in the vaporizer minimize.Normally, the product that per hour accumulates in the vaporizer is lower than 2%.Preferably, the product that per hour is accumulated in the vaporizer is lower than 1%.If the concentrated liquid product that per hour is accumulated in the falling film evaporator is lower than 0.5%, then security can be improved.
Falling film evaporator of the present invention adopts a kind of heating medium to heat.It can be and is generally used for the medium that conducts heat arbitrarily.For example, this medium can be hot water or steam, and its circulation enters into described vaporizer.Advantageously, it is a hot water.Usually, described vaporizer is heated to above from 20 ℃ of the high boiling point liquid fraction vaporization temperatures of still-process.Preferably, it only is heated to above 10 ℃ of this temperature.
In falling film evaporator of the present invention, the high boiling point liquid fraction of solution flows downward under action of gravity, and described thermal medium logistics and the steam logistics that is produced by it can flow downward, and also can upwards flow.Preferably, hot water circulation is as heating medium, and the high boiling point liquid fraction of described hot water, described solution and the steam that is produced by it flow downward simultaneously.
Flow out the concentrated solution of described falling film evaporator, advantageously it is cooled off in storage or before using.For this purpose, it can be transferred in the water cooler.This transfer can be operated through a divider under action of gravity.Concentrated solution is transferred to wherein water cooler, be preferably a kind of falling film type water cooler.Described water cooler can be the medium that is usually used in arbitrarily conducting heat and cools off.Preferably, described heat-eliminating medium is water and/or ethylene glycol.In described water cooler, concentrated solution is cooled to be lower than 15 ℃ usually.Preferably be cooled to about 0 ℃.
Concentrated solution of the present invention is dissolved in by a kind of compound that concentrated solution in a kind of solvent forms, and this solvent has lower boiling point than this compound.This compound at high temperature and/or to be present in high density may be unsettled in the solvent.Usually, described solvent is a water.Hydrogen peroxide is a kind of unstable product that is suitable for very much the inventive method.Therefore, the present invention is particularly suitable for spissated aqueous hydrogen peroxide solution.
Be fed to the dilute hydrogen peroxide aqueous solution in the rectifying column, contain the hydrogen peroxide up to 70%w/w usually, still, it also can contain the hydrogen peroxide up to 86%w/w.This dilute hydrogen peroxide preferably only contains the organism and the metal of trace.Normally, it contains the organism that is lower than 100mg/kg.Metal in this dilute solution contains and preferably is lower than 1mg/kg.The superoxol of this purity can obtain by any known purification process.For example, it can prepare by a kind of pair of distillating method.For example, it comprises first, and to be distilled to concentration be 70%, then with the softening water dilution, last, carries out after-fractionating to obtain needed concentration.
By the resulting concentrated superoxol of the evaporation of the high boiling point liquid fraction in the described falling film evaporator, contain the hydrogen peroxide of 80%w/w at least usually.It can contain the hydrogen peroxide up to 90%w/w.Adopt method of the present invention, can obtain concentration and be 98% hydrogen peroxide.In some cases, in addition the hydrogen peroxide of 100%w/w concentration also can obtain.
It also is not that commodity can get so far that concentration of hydrogen peroxide is higher than 90%w/w, and this is because its product has danger.Therefore, the invention still further relates to the concentrated hydration superoxol that is obtained by aforesaid method, its concentration is at least 90%w/w.
Description of drawings
Fig. 1 is the synoptic diagram of apparatus of the present invention.
Embodiment
Method of the present invention will be further described in following specification sheets, can be referring to Fig. 1, and it is the synoptic diagram of apparatus of the present invention preferred embodiment.
Described distillation column (1) contains a packed column of operating (structured packing-SULZER BX type) under vacuum.Selecting for use of this filler can allow each theoretical level of separating to have lower pressure drop, and therefore, it can limit near-bottom temperature.A kind of Dilute Hydrogen Peroxide Solution is fed to the middle part of this post through inlet duct (2).Subsequently, the first half of this post (3) is as an enrichment region, and this post than lower part (4) as stripping zone, it can reduce the energy requirement and total amount (liquid gathering) requirement of this method.
The capital steam is transported in the condenser (6) through pipeline (5).Resulting liquid and steam are transported in the liquid separator (8) through pipeline (7).With the part recovering liquid among pipeline (9) is back to the top of post (1).Uncondensable gas adopts vacuum system to remove.
In the resulting high boiling point liquid fraction of distillation column (1) bottom, be transported to continuously in the described falling film evaporator (11) through divider (10).Use falling film evaporator of the present invention, can reduce the residence time of concentrated hydrogen peroxide under the high temperature, like this, just can make the danger of explosive decomposition reach minimum.It also can guarantee liquid dispersion on the surface, rather than exists with bulk form, and it can make the possibility of blast reach minimum.At last, it can make the temperature rise of evaporative process minimize, thereby the danger of explosive decomposition is minimized.Adopt the gravity flowage mode heat that can avoid friction to become the danger of explosive decomposition starting resource.Therefore, method of the present invention can advantageously be used for preparing spissated explosive solution.
The resulting concentrated solution of bottom at falling film evaporator (11) is transported in the vapour/liquid separator (13) through pipeline (12).Steam is sent back to the bottom of this post through pipeline (14).Final liquid product is transported in the falling film type water cooler (16) through pipeline (15) continuously, and this water cooler has best heat transfer coefficient and minimum liquid hold-up.
This water cooler (16) can make spent glycol as refrigerant, preferably has reverse flow configuration.
Cooled the finished product emit through pipeline (17).
Embodiment 1Prepare a kind of Dilute Hydrogen Peroxide Solution
H with 35-42%
2O
2Solution feed is in first distillation procedure, and it is positioned at the bottom of the distillation column that contains 3-5 theoretical tray.
This post is to be that 57-74 ℃ (135-165) and column top temperature are 43-60 ℃ (110-140 °F) in the suspension column temperature, and suspension column pressure is 0.075-0.15 crust (30-60 inch of water), and reflux ratio is to operate under the condition of 0.25-0.35.
It is 45-49% that distillment is diluted to concentration with ultrapure water.Then in a glass distillation column, be distilled to the H that concentration is 50-74% again
2O
2W/w.The glass distillation column is a packed column, and its theoretical plate number is 2-4, and it is to operate under temperature 57-69 ℃ (135-157) and suspension column pressure 0.05-0.11 crust (20-43 inch of water) and reflux ratio are the condition of 0.05-0.12.
Final superoxol has the TOC charging of about 10-20%, the negatively charged ion of 0.1%-1% and the positively charged ion of about 0.5-2%.
Embodiment 2Prepare a kind of concentrated superoxol of the present invention
Adopt a kind of as shown in Figure 1 device (difference is water cooler, it be a kind of for heating jacket institute around coiled pipe, alternative falling film type water cooler), be used for preparing the superoxol of 96%w/w according to following step.
With the middle part of 86%w/w solution feed to a filling distillation column, it contains 4-5 theoretical tray.
The internal diameter of this distillation column fill area is 75mm, and total height is 1.42m.It is in near-bottom temperature about 40 ℃, and about 18 ℃ of head temperature, the vacuum of 8-10 millibar and reflux ratio are to operate under 1: 1 the condition.
The high boiling fraction of solution is transported in the falling film evaporator through divider.
This falling film evaporator is made up of by the single sleeve pipe that adds of 750mm an about 25mm of diameter and total height.Water enters into described chuck 65 ℃ of circulations.At the bottom of this falling film evaporator, a water cooler is arranged, it by one by chuck around coiled pipe formed, its used water is cooled off.
When feeding rate was 360g/h, speed that can about 300g/h obtained the superoxol product of 96%w/w.
Claims (8)
1. method that concentrates the dilute solution contain solvent, comprising the distilation steps in distillation column, and the evaporation step in falling film evaporator subsequently, wherein said distillation column and described falling film evaporator are distinct and form with the device feature that divider separates by two, and wherein said distillation column is mounted on the top layer of described falling film evaporator, and this method may further comprise the steps:
(a) a certain position on distillation column or a plurality of position input dilute solution;
(b) in this distillation column, distill described dilute solution, obtain the lower boiling gaseous fraction of solution at the top of described distillation column, obtain the high boiling point liquid fraction of solution in the bottom of described distillation column;
(c), the high boiling point liquid fraction of described solution is transferred to the described falling film evaporator from described distillation column bottom through divider;
(d) the high boiling point liquid fraction of concentrated described solution in described falling film evaporator;
(e) collect spissated solution in the bottom of described falling film evaporator;
(f) effusive concentrated solution cools off in water cooler among a divider is transported to a water cooler in the described falling film evaporator,
Wherein said spissated solution is spissated aqueous hydrogen peroxide solution.
According to the process of claim 1 wherein described distillation column and described falling film evaporator the axle in line.
3. according to the method for claim 1 or 2, wherein the divider in described step (c) its cross-sectional area at narrow place less than the cross-sectional area of described distillation column.
4. according to the method for claim 1 or 2, wherein said distillation column and described falling film evaporator are to adopt to allow the high boiling point liquid fraction to assemble from the mode that described distillation column flows to the described falling film evaporator under action of gravity.
5. according to the method for claim 1 or 2, wherein said distillation is to carry out under peak pressure is the condition of 10 torrs.
6. according to the method for claim 1 or 2, wherein said falling film evaporator by one by chuck around pipe form, and circulating hot water heats described pipe in described chuck.
7. according to the method for claim 6, wherein hot water in described chuck and the high boiling point liquid fraction in described pipe flow downward simultaneously.
8. according to the process of claim 1 wherein that effusive concentrated solution contains the hydrogen peroxide of 90%w/w at least from described falling film evaporator.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP99307848A EP1090663A1 (en) | 1999-10-05 | 1999-10-05 | Process for the manufacture of concentrated solutions |
| EP99307848.4 | 1999-10-05 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1291521A CN1291521A (en) | 2001-04-18 |
| CN1185036C true CN1185036C (en) | 2005-01-19 |
Family
ID=8241659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001333569A Expired - Fee Related CN1185036C (en) | 1999-10-05 | 2000-10-05 | Method for preparing concentrated solution |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US6780288B1 (en) |
| EP (1) | EP1090663A1 (en) |
| CN (1) | CN1185036C (en) |
| FR (1) | FR2799136B1 (en) |
| RU (1) | RU2241660C2 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1318679B1 (en) * | 2000-08-11 | 2003-08-27 | Enichem Spa | PROCESS FOR THE PRODUCTION OF OXYGEN WATER. |
| DE10144013A1 (en) * | 2001-09-07 | 2003-03-27 | Basf Ag | Working up aqueous hydrogen peroxide solution from direct synthesis, useful e.g. in chemical synthesis, bleaching paper and pulp, sewage treatment or chemical polishing fluid, uses evaporator cascade with continuous evaporator at end |
| CN100347078C (en) * | 2004-09-27 | 2007-11-07 | 上海哈勃化学技术有限公司 | Hydrogen peroxide concentration process |
| CN102161475A (en) * | 2009-11-02 | 2011-08-24 | 郑国玉 | Concentration method in production of hydrogen peroxide by anthraquinone method |
| DE102010039748A1 (en) * | 2010-08-25 | 2012-03-01 | Evonik Degussa Gmbh | Process for concentrating aqueous hydrogen peroxide solution |
| CN102174371B (en) * | 2011-02-16 | 2012-12-26 | 山东省科学院能源研究所 | Process method and device for coupling acetone-butyl alcohol fermentation and separation |
| CN102151412B (en) * | 2011-02-16 | 2013-05-08 | 山东省科学院能源研究所 | Process and device for distilling and concentrating solution |
| US9213341B2 (en) | 2012-10-12 | 2015-12-15 | American Sterilizer Company | Biological safety cabinet with a falling-film evaporator |
| PL403721A1 (en) | 2013-04-30 | 2014-11-10 | Instytut Lotnictwa | Method for preparing hydrogen peroxide, in particular HTP class for uses in the drive systems for the vacuum distillation |
| FR3024459B1 (en) * | 2014-07-30 | 2018-04-13 | Ifp Energies Now | METHOD FOR FRACTIONING HYDROCARBON LOADS USING A DEVICE COMPRISING PERMUTABLE BACKGROUND AREAS |
| PL233084B1 (en) | 2015-07-14 | 2019-08-30 | Inst Lotnictwa | Single-stage method for obtaining HTP ( High Test Peroxide) class hydrogen peroxide for the driving applications and the system for obtaining it |
| CN113289364B (en) * | 2021-05-18 | 2023-04-11 | 重庆宏大化工科技有限公司 | Concentrating device for hydrogen peroxide production and using method thereof |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB590439A (en) * | 1945-04-17 | 1947-07-17 | Laporte Ltd B | Improvements in and relating to the concentration and purification of hydrogen peroxide by distillation |
| GB668874A (en) | 1948-07-30 | 1952-03-26 | Produits Peroxydes Soc D | Improvements relating to the manufacture of high concentrated hydrogen peroxide solutions by rectification of diluted solutions |
| NL94445C (en) * | 1952-04-24 | |||
| BE756015A (en) * | 1969-09-10 | 1971-02-15 | Degussa | PROCESS FOR THE PREPARATION OF HYDROGEN PEROXIDE (E) |
| EG11268A (en) * | 1972-07-26 | 1977-08-15 | Krupp Ag Huettenwerke | Method and apparatus for producing distillate |
| IT1027410B (en) * | 1974-02-25 | 1978-11-20 | Degussa | CONTINUOUS PROCEDURE FOR THE PRODUCTION OF GLYCIDE |
| US4328074A (en) * | 1980-11-12 | 1982-05-04 | Resources Conservation Company | Production of concentrated alcohol and distillery slop |
| CN85103225B (en) * | 1985-04-01 | 1988-09-28 | 化学工业部黎明化工研究院 | Purification and concentration of h202 |
| ES2194965T3 (en) | 1996-10-09 | 2003-12-01 | Sulzer Chemtech Ag | DISTILLATION INSTALLATION. |
| US6290820B1 (en) * | 1997-12-17 | 2001-09-18 | Iowa State University Research Foundation, Inc. | Apparatus and method for concentrating a dilute solution |
| EP0933107B1 (en) * | 1998-01-30 | 2005-10-26 | Ube Industries, Ltd. | Process for refining heat-deteriorative compound, contained in multi-component liquid mixture, by distillation |
| DE19916753C1 (en) * | 1999-04-14 | 2000-07-06 | Krupp Uhde Gmbh | Production of 1,2-dichloroethane, used in the manufacture of vinyl chloride, by reaction of chlorine and ethylene in plant including a downdraft evaporator |
-
1999
- 1999-10-05 EP EP99307848A patent/EP1090663A1/en not_active Withdrawn
-
2000
- 2000-10-03 FR FR0012764A patent/FR2799136B1/en not_active Expired - Fee Related
- 2000-10-04 RU RU2000125113/15A patent/RU2241660C2/en not_active IP Right Cessation
- 2000-10-05 US US09/679,646 patent/US6780288B1/en not_active Expired - Fee Related
- 2000-10-05 CN CNB001333569A patent/CN1185036C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| US6780288B1 (en) | 2004-08-24 |
| FR2799136B1 (en) | 2002-07-19 |
| RU2241660C2 (en) | 2004-12-10 |
| EP1090663A1 (en) | 2001-04-11 |
| CN1291521A (en) | 2001-04-18 |
| FR2799136A1 (en) | 2001-04-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1185036C (en) | Method for preparing concentrated solution | |
| US10384146B2 (en) | Divided wall distillation column | |
| JP4620694B2 (en) | Method for producing high purity trichlorosilane | |
| CN101607908B (en) | Process for preparing diaryl carbonates from dialkyl carbonates | |
| CN105749575B (en) | The divided-wall distillation column of tail gas absorption liquid and condensate liquid recovery in production of polysilicon, method, processing system | |
| CN1143623A (en) | Separation of (meth) acrylic acid from reaction gas mixture formed in catalytic gas phase oxidation of C3/C4 compounds | |
| JP5362331B2 (en) | Method for purifying diaryl carbonate | |
| US20090321057A1 (en) | Column Installed Condenser | |
| KR20130111406A (en) | Heat integrated distillation apparatus | |
| CN1125306C (en) | Method for producing oxygen | |
| CN101028918A (en) | Recovery of hydrofluoric acid | |
| CN109320417A (en) | Utilize the device and method of partition tower purification Ergol | |
| CN1106562C (en) | Cryogenic rectification system for producing multi-purity oxygen | |
| TWI373461B (en) | ||
| CN218248558U (en) | Distillation column equipment | |
| US10281209B2 (en) | Heat exchangers for low temperature carbon dioxide separation from natural gas | |
| JP2001009201A (en) | Apparatus and method for purification by distillation | |
| TWI584860B (en) | An evaporator and process for use thereof | |
| RU2393347C1 (en) | Oil treatment method | |
| CN220633052U (en) | Purification system of 2, 6-xylenol | |
| CN107541339B (en) | Product fractionation device and process for biodiesel | |
| EP3106214B1 (en) | Gas stripper system | |
| CN101036840A (en) | Full effective tray with separating phase transformation and small plate distance rectifying tower | |
| US4484985A (en) | Distillation and condensing process | |
| CN215841685U (en) | Chloroethylene high-boiling substance treatment system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |